CN110282947B - High-strength composite aerogel thermal insulation material and preparation method thereof - Google Patents
High-strength composite aerogel thermal insulation material and preparation method thereof Download PDFInfo
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- CN110282947B CN110282947B CN201910512011.0A CN201910512011A CN110282947B CN 110282947 B CN110282947 B CN 110282947B CN 201910512011 A CN201910512011 A CN 201910512011A CN 110282947 B CN110282947 B CN 110282947B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention discloses a high-strength composite aerogel thermal insulation material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed and stirred, then the pH is adjusted, and silica sol is obtained by hydrolysis; (2) adding carbon nitride fibers and aluminum silicate fibers into the prepared silicon dioxide sol, adjusting the pH, uniformly dispersing, standing and aging to obtain a composite wet gel; (3) soaking the composite wet gel in a sodium bicarbonate aqueous solution for solvent replacement; (4) and taking out the composite wet gel after the solvent replacement, and drying to obtain the composite aerogel thermal insulation material. According to the invention, the carbon nitride fibers are uniformly distributed on the surface or inside the aerogel, so that the mechanical property of the silicon dioxide aerogel is effectively improved; in addition, the invention utilizes the softness and the heat insulation performance of the aluminum silicate fiber to modify the silicon dioxide aerogel, enhances the flexibility and reduces the heat conductivity coefficient, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of aerogel preparation, and particularly relates to a high-strength composite aerogel thermal insulation material and a preparation method thereof.
Background
The aerogel is a light nano solid material which is formed by mutually gathering nano-scale ultrafine particles to form a nano porous network structure and is filled with gaseous dispersion media in network pores. The porosity is as high as 99.8%, the typical size of the pores is 1-40nm, and the specific surface area is 400-2In terms of/g, and a density as low as 3kg/m3The heat conductivity coefficient at room temperature can be as low as below 0.010W/(m.K), and the light-weight, light-transmitting, heat-insulating, heat-preserving, sound-insulating, fireproof and impact-resistant light-weight material has excellent chemical stability and non-inflammability. Due to the characteristics, the silica aerogel material has wide application potential in the aspects of thermal, acoustic, optical, microelectronic, particle detection and the like.
The unique nano-porous structure of the silica aerogel material enables the pore diameter to be smaller than the average free path of gas molecules, so that the convective heat transfer of the gas molecules is limited, meanwhile, the solid phase heat transfer of the material is limited due to the ultrahigh porosity, and in addition, the high-temperature radiation heat transfer of the material can be reduced by adding a proper amount of infrared opacifier, so that the silica aerogel is regarded as a solid material with the best heat insulation performance at present and has wide application prospect in the field of heat insulation materials.
Chinese patent CN 108821740a discloses a silica aerogel-carbon fiber composite thermal insulation material, which is made of silica aerogel, carbon fiber, water, diatomite and pure acrylic emulsion, and solves some problems of silica aerogel in the prior art to a certain extent, but the comprehensive performance of the material cannot reach the satisfactory level of industrial application, and it is still necessary to develop a composite aerogel material with high strength and excellent thermal insulation performance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-strength composite aerogel thermal insulation material.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a high-strength composite aerogel thermal insulation material comprises the following steps:
(1) tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed and stirred for a period of time, then hydrochloric acid solution is added to regulate the pH value, and silica sol is prepared by hydrolysis;
(2) adding carbon nitride fibers and aluminum silicate fibers into the silicon dioxide sol prepared in the step (1), adjusting the pH to 6-8, uniformly dispersing, sealing, standing and aging the silicon dioxide sol to obtain a composite wet gel;
(3) soaking the composite wet gel in the step (2) in a sodium bicarbonate aqueous solution for solvent replacement;
(4) and taking out the composite wet gel after the solvent replacement, and fully drying to obtain the high-strength composite aerogel thermal insulation material.
Preferably, the stirring time in step (1) is about 2.5h, the pH is adjusted to about 3 by adding hydrochloric acid, and the hydrolysis temperature is about 40-60 ℃.
Preferably, the mole ratio of the tetraethyl orthosilicate, the absolute ethyl alcohol and the deionized water in the step (1) is 1:8-12: 2-6.
Preferably, the addition amount of the carbon nitride fiber in the step (2) is 1-2 wt% of the silica sol, and the addition amount of the aluminum silicate fiber is 3-6 wt% of the silica sol.
Preferably, the concentration of the sodium bicarbonate aqueous solution in the step (3) is 0.1-0.2 g/mL.
Preferably, the drying in the step (4) is drying at 60-80 ℃ for 10-15 min, washing with deionized water, and drying at 100-250 ℃.
In addition, the invention also claims the high-strength composite aerogel thermal insulation material prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the strength and toughness of the silicon dioxide aerogel are modified by using the carbon nitride fibers, and the carbon nitride fibers are uniformly distributed on the surface or inside the aerogel, so that the mechanical property of the silicon dioxide aerogel is effectively improved; in addition, the aluminum silicate fibers are added in the preparation process of the aerogel, and the silicon dioxide aerogel is modified by utilizing the softness and the heat insulation performance of the aluminum silicate fibers, so that the flexibility of the silicon dioxide aerogel is enhanced, and the heat conductivity coefficient of the silicon dioxide aerogel is reduced to a certain extent.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
A preparation method of a high-strength composite aerogel thermal insulation material comprises the following steps:
(1) at room temperature, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed according to a molar ratio of 1: 10: 5, mixing, stirring for 2.5h, then adding a hydrochloric acid solution to adjust the pH value to be about 3, and hydrolyzing at 50 ℃ to obtain silicon dioxide sol;
(2) taking 60 parts of the silica sol prepared in the step (1), adding 1 part of carbon nitride fiber and 2.4 parts of aluminum silicate fiber, adjusting the pH to be about 7, uniformly dispersing by ultrasonic stirring, sealing and standing the silica sol to obtain a composite wet gel;
(3) adding 50 parts of absolute ethyl alcohol into the composite wet gel obtained in the step (2), sealing, placing in a water bath kettle at 20 ℃, standing, aging for 24 hours, and then soaking in a sodium bicarbonate aqueous solution of 0.15g/mL for solvent replacement for 12 hours;
(4) and taking out the composite wet gel after solvent replacement, drying at 70 ℃ for 12min, cleaning with deionized water, and drying at 120 ℃ for 12h to obtain the high-strength composite aerogel thermal insulation material.
Example 2
A preparation method of a high-strength composite aerogel thermal insulation material comprises the following steps:
(1) at room temperature, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed according to a molar ratio of 1: 8: 4, mixing, stirring for 2.5h, then adding a hydrochloric acid solution to adjust the pH value to be about 3, and hydrolyzing at 50 ℃ to obtain silicon dioxide sol;
(2) taking 60 parts of the silica sol prepared in the step (1), adding 0.9 part of carbon nitride fiber and 2 parts of aluminum silicate fiber into the silica sol, adjusting the pH to be about 7, uniformly dispersing the mixture by ultrasonic stirring, and sealing and standing the silica sol to obtain a composite wet gel;
(3) adding 50 parts of absolute ethyl alcohol into the composite wet gel obtained in the step (2), sealing, placing in a water bath kettle at 20 ℃, standing, aging for 24 hours, and then soaking in a sodium bicarbonate aqueous solution of 0.10g/mL for solvent replacement for 12 hours;
(4) and taking out the composite wet gel after solvent replacement, drying at 70 ℃ for 12min, cleaning with deionized water, and drying at 120 ℃ for 12h to obtain the high-strength composite aerogel thermal insulation material.
Example 3
A preparation method of a high-strength composite aerogel thermal insulation material comprises the following steps:
(1) at room temperature, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed according to a molar ratio of 1: 9: 4, mixing, stirring for 2.5h, then adding a hydrochloric acid solution to adjust the pH value to be about 3, and hydrolyzing at 50 ℃ to obtain silicon dioxide sol;
(2) taking 60 parts of the silica sol prepared in the step (1), adding 1.2 parts of carbon nitride fibers and 3 parts of aluminum silicate fibers, adjusting the pH to be about 7, uniformly stirring and dispersing by ultrasonic waves, and sealing and standing the silica sol to obtain a composite wet gel;
(3) adding 50 parts of absolute ethyl alcohol into the composite wet gel obtained in the step (2), sealing, placing in a water bath kettle at 20 ℃, standing, aging for 24 hours, and then soaking in a sodium bicarbonate aqueous solution of 0.12g/mL for solvent replacement for 12 hours;
(4) and taking out the composite wet gel after solvent replacement, drying at 70 ℃ for 12min, cleaning with deionized water, and drying at 120 ℃ for 12h to obtain the high-strength composite aerogel thermal insulation material.
Example 4
A preparation method of a high-strength composite aerogel thermal insulation material comprises the following steps:
(1) at room temperature, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed according to a molar ratio of 1: 10: 5, mixing, stirring for 2.5h, then adding a hydrochloric acid solution to adjust the pH value to be about 3, and hydrolyzing at 50 ℃ to obtain silicon dioxide sol;
(2) taking 60 parts of the silica sol prepared in the step (1), adding 0.6 part of carbon nitride fiber and 1.8 parts of aluminum silicate fiber into the silica sol, adjusting the pH to be about 7, uniformly dispersing the mixture by ultrasonic stirring, and sealing and standing the silica sol to obtain a composite wet gel;
(3) adding 50 parts of absolute ethyl alcohol into the composite wet gel obtained in the step (2), sealing, placing in a water bath kettle at 20 ℃, standing, aging for 24 hours, and then soaking in a sodium bicarbonate aqueous solution of 0.16g/mL for solvent replacement for 12 hours;
(4) and taking out the composite wet gel after solvent replacement, drying at 70 ℃ for 12min, cleaning with deionized water, and drying at 120 ℃ for 12h to obtain the high-strength composite aerogel thermal insulation material.
Example 5
A preparation method of a high-strength composite aerogel thermal insulation material comprises the following steps:
(1) at room temperature, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed according to a molar ratio of 1: 10: 4, mixing, stirring for 2.5h, then adding a hydrochloric acid solution to adjust the pH value to be about 3, and hydrolyzing at 50 ℃ to obtain silicon dioxide sol;
(2) taking 60 parts of the silica sol prepared in the step (1), adding 0.8 part of carbon nitride fiber and 2 parts of aluminum silicate fiber into the silica sol, adjusting the pH to be about 7, uniformly dispersing the mixture by ultrasonic stirring, and sealing and standing the silica sol to obtain a composite wet gel;
(3) adding 50 parts of absolute ethyl alcohol into the composite wet gel obtained in the step (2), sealing, placing in a water bath kettle at 20 ℃, standing, aging for 24 hours, and then soaking in a sodium bicarbonate aqueous solution of 0.15g/mL for solvent replacement for 12 hours;
(4) and taking out the composite wet gel after solvent replacement, drying at 70 ℃ for 12min, cleaning with deionized water, and drying at 120 ℃ for 12h to obtain the high-strength composite aerogel thermal insulation material.
Example 6
A preparation method of a high-strength composite aerogel thermal insulation material comprises the following steps:
(1) at room temperature, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed according to a molar ratio of 1: 12: 6, mixing, stirring for 2.5h, then adding a hydrochloric acid solution to adjust the pH value to be about 3, and hydrolyzing at 50 ℃ to obtain silicon dioxide sol;
(2) taking 60 parts of the silica sol prepared in the step (1), adding 1 part of carbon nitride fiber and 2 parts of aluminum silicate fiber, adjusting the pH to be about 7, uniformly stirring and dispersing by ultrasonic waves, and sealing and standing the silica sol to obtain a composite wet gel;
(3) adding 50 parts of absolute ethyl alcohol into the composite wet gel obtained in the step (2), sealing, placing in a water bath kettle at 20 ℃, standing, aging for 24 hours, and then soaking in a sodium bicarbonate aqueous solution of 0.15g/mL for solvent replacement for 12 hours;
(4) and taking out the composite wet gel after solvent replacement, drying at 70 ℃ for 12min, cleaning with deionized water, and drying at 120 ℃ for 12h to obtain the high-strength composite aerogel thermal insulation material.
Comparative example 1
A preparation method of a high-strength composite aerogel thermal insulation material comprises the following steps:
(1) at room temperature, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed according to a molar ratio of 1: 10: 5, mixing, stirring for 2.5h, then adding a hydrochloric acid solution to adjust the pH value to be about 3, and hydrolyzing at 50 ℃ to obtain silicon dioxide sol;
(2) taking 60 parts of the silica sol prepared in the step (1), adding 2.4 parts of aluminum silicate fiber into the silica sol, adjusting the pH to be about 7, ultrasonically stirring the mixture uniformly, and then sealing and standing the silica sol to obtain a composite wet gel;
(3) adding 50 parts of absolute ethyl alcohol into the composite wet gel obtained in the step (2), sealing, placing in a water bath kettle at 20 ℃, standing, aging for 24 hours, and then soaking in a sodium bicarbonate aqueous solution of 0.15g/mL for solvent replacement for 12 hours;
(4) and taking out the composite wet gel after solvent replacement, drying at 70 ℃ for 12min, cleaning with deionized water, and drying at 120 ℃ for 12h to obtain the high-strength composite aerogel thermal insulation material.
Comparative example 2
A preparation method of a high-strength composite aerogel thermal insulation material comprises the following steps:
(1) at room temperature, tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed according to a molar ratio of 1: 10: 5, mixing, stirring for 2.5h, then adding a hydrochloric acid solution to adjust the pH value to be about 3, and hydrolyzing at 50 ℃ to obtain silicon dioxide sol;
(2) taking 60 parts of the silica sol prepared in the step (1), adding 1 part of carbon nitride fibers into the silica sol, adjusting the pH value to be about 7, uniformly dispersing the mixture by ultrasonic stirring, and sealing and standing the silica sol to obtain a composite wet gel;
(3) adding 50 parts of absolute ethyl alcohol into the composite wet gel obtained in the step (2), sealing, placing in a water bath kettle at 20 ℃, standing, aging for 24 hours, and then soaking in a sodium bicarbonate aqueous solution of 0.15g/mL for solvent replacement for 12 hours;
(4) and taking out the composite wet gel after solvent replacement, drying at 70 ℃ for 12min, cleaning with deionized water, and drying at 120 ℃ for 12h to obtain the high-strength composite aerogel thermal insulation material.
To illustrate the performance of the composite aerogel insulation materials prepared according to the present invention, the performance of the composite aerogel insulation materials prepared according to examples 1-6 and comparative examples 1-2 was measured, and the results are shown in the following table:
as can be seen from the above table 1, the composite aerogel thermal insulation material prepared by the invention shows good performance, and the thermal conductivity coefficient is less than 0.02W/(m)2K) while the flexural strength and tensile strength are both higher and significantly higher than comparative examples 1 and 2.
The above-mentioned embodiments are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only the most preferred embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions, equivalents, etc. made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (6)
1. The preparation method of the high-strength composite aerogel thermal insulation material is characterized by comprising the following steps of:
(1) tetraethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed and stirred for a period of time, then hydrochloric acid solution is added to regulate the pH value, and silica sol is prepared by hydrolysis;
(2) adding carbon nitride fibers and aluminum silicate fibers into the silicon dioxide sol prepared in the step (1), adjusting the pH to 6-8, uniformly dispersing, sealing, standing and aging the silicon dioxide sol to obtain a composite wet gel;
(3) soaking the composite wet gel in the step (2) in a sodium bicarbonate aqueous solution for solvent replacement;
(4) taking out the composite wet gel after solvent replacement, and fully drying to obtain the high-strength composite aerogel thermal insulation material;
wherein, the adding amount of the carbon nitride fiber in the step (2) is 1-2 wt% of the silica sol, and the adding amount of the aluminum silicate fiber is 3-6 wt% of the silica sol.
2. The method according to claim 1, wherein the stirring time in step (1) is 2.5 hours, the pH is adjusted to 3 by adding hydrochloric acid, and the hydrolysis temperature is 40-60 ℃.
3. The method according to claim 1, wherein the molar ratio of tetraethyl orthosilicate, absolute ethanol and deionized water in step (1) is 1:8-12: 2-6.
4. The method according to claim 1, wherein the concentration of the aqueous solution of sodium bicarbonate in step (3) is 0.1 to 0.2 g/mL.
5. The preparation method according to claim 1, wherein the drying in the step (4) is drying at 60-80 ℃ for 10-15 min, washing with deionized water, and drying at 100-250 ℃.
6. A high strength composite aerogel thermal insulation material prepared by the preparation method of any one of claims 1 to 5.
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| CN114195495A (en) * | 2020-10-17 | 2022-03-18 | 朱晶晶 | Silica aerogel composite thermal insulation fabric |
| CN114622442B (en) * | 2021-07-05 | 2023-06-16 | 重庆大学 | Novel insulating paper material and preparation method and application thereof |
| CN114574085B (en) * | 2022-03-10 | 2023-02-10 | 山东沃丰新材料有限公司 | Heat-insulation color aluminum plate and processing technology |
| CN115974520B (en) * | 2023-02-07 | 2023-07-25 | 河南冠合新材料科技有限公司 | Preparation method of chopped carbon fiber composite material |
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